III / WHISKY: DISTILLATION 4485
WHISKY: DISTILLATION
D. S. Pickerell, Maker’s Mark Distillery,
Loretto, KY, USA
Copyright ^ 2000 Academic Press
Introduction
Grain fermentation yields a water-based liquid mix-
ture commonly referred to as distiller’s beer. This
beer will typically contain between 5 and 9% by
weight ethyl alcohol, 6}8% by weight residual grain
solids, and a very small quantity of other compounds
known as fusel oils. These fusel oils, also known as
congeners, are primarily higher alcohols that are sol-
uble in ethyl alcohol but only partially soluble in
water. The congeners contribute to the taste and
aroma of whisky and are not typically removed in
a single-column distillation.
All separation technologies exploit some difference
between items in a mixture or solution in order
to cause them to separate. These differences may
be physical, chemical or electrical in nature. In
particular, distillation takes advantage of the differ-
ence in boiling points to separate soluble liquids from
one another. Not all liquid solutions may be eco-
nomically separable by distillation for a variety of
reasons. For example, one or more of the liquid
components may not appreciably volatize, or the
change in the concentrations of the components be-
tween the gas phase and the liquid phase may be so
small that the process becomes impractical. It may
even happen that there is no change in the composi-
tion whatsoever.
In general, during distillation of completely
miscible liquids, the component with the
higher boiling point moves toward the bottom of
the still while the component with the lower boil-
ing point moves toward the top. In whisky produc-
tion, water boils at a higher temperature while
ethyl alcohol boils at a lower temperature. As a
result, distillation has an added beneRt as the
separation technique of choice, because the grain
residue is naturally carried to the bottom of the
still along with the water. If the still is
properly designed, the concentration of alcohol
in the still bottoms should be negligible and the
discharge from the bottom of the still will contain
all of the unwanted grain residues and the excess
water.
Vapour^Liquid Equilibrium
In order to understand what happens during the dis-
tillation process, we need to address the topic of
vapour}liquid equilibrium. For the purpose of this
discussion, we will consider the case of distilling
a mixture of water and ethyl alcohol at a constant
pressure of 1 atm. Figure 1 shows the vapour}liquid
equilibrium curves for this mixture. It should be
noted that the concept of a single boiling point is
invalid for this type of solution. The lower line is
referred to as the bubble point line. At a given concen-
tration of ethyl alcohol in a liquid mixture of ethanol
and water, the bubble point line indicates the temper-
ature at which the Rrst bubble of vapour forms as the
solution is heated. The upper line is called the dew
point line. At a given concentration of ethanol in
a vapour mixture of ethanol and water, the dew point
line indicates the temperature at which the Rrst drop
of condensate is formed as the mixture is cooled.
In order to explain the distillation process, a rather
simplistic approach is employed by assuming an
absolutely ideal system with no inefRciencies. For
actual distillation system design, a much more thor-
ough analysis would need to be done. For illustrative
purposes, let us assume we have a liquid solution
consisting of 40% by weight ethanol and 60% by
weight water in a pot at 823C. Figure 2 shows the
vapour-liquid equilibrium of this solution, which is
currently at point A. Let us further assume that we
will add heat to this pot in an effort to bring the
temperature up to 993C, as represented by point
B (Figure 3). The solution will heat up until the
Figure 1 Vapour}liquid equilibrium: ethanol}water, 760 mmHg.
Continuous line, bubble point line; dashed line, dew point line.
4486 III / WHISKY: DISTILLATION
Figure 2 Vapour}liquid equilibrium: ethanol}water, 760 mmHg.
Continuous line, bubble point line; dashed line, dew point line.
temperature reaches about 833C where the heating
line intersects the bubble point line at point M. At this
point, the Rrst bubble of vapour forms, but because
the ethanol vaporizes more easily than the water at
this point, the vapour phase is enriched in ethanol.
The concentration of ethanol in this Rrst bubble of
vapour is found at point N, about 75% ethanol by
weight (Figure 4). As the mixture continues to heat
up, eventually point P is reached at about 873C. At
this point, the mixture is boiling. The liquid still in the
pot has a concentration of about 17%, as indicated
by point 0, while the total vapour concentration is
represented by point R at about 64% ethanol (Fig-
ure 5). The solution can continue to be heated until
the heating line intersects with the dew point line at
point T. At this point there is only one drop of liquid
left in the pot and its concentration is found at point
S to be about 2% ethanol by weight. If all of the
vapour from this experiment was collected, its con-
centration would be found at point T } approxim-
ately 40% by weight ethanol } right back where we
Figure 3 Vapour}liquid equilibrium: ethanol}water, 760 mmHg.
Continuous line, bubble point line; dashed line, dew point line.
Figure 4 Vapour}liquid equilibrium: ethanol}water, 760 mmHg.
Continuous line, bubble point line; dashed line, dew point line.
started from, only hotter. The vapour could then be
superheated to 993C at point B, but no further cha-
nges in ethanol concentration would occur.
It should be noted that, during the distillation pro-
cess, once the bubble line is reached, the concentra-
tion of ethanol in the liquid phase moves along the
bubble point line from left to right, constantly de-
creasing until the supply of liquid is exhausted. Sim-
ilarly, the concentration of ethanol in the vapour
phase also decreases, along the dew point line, as the
liquid in the pot is exhausted. As a result, if we were
going to distill ethanol from water in a batch process
with a lower limit of acceptable proof, we would
have to stop the process before all the ethanol
could be recovered. Ideally, we would like to be
able to recover all of the ethanol from the solution at
some speciRed constant proof. If point N is the target,
we could devise a process where we continually
replenish the liquid in the pot at 40% ethanol and
a rate equal to the rate that product is taken off by
condensation.
Figure 5 Vapour}liquid equilibrium: ethanol}water, 760 mmHg.
Continuous line, bubble point line; dashed line, dew point line.

Figure 6 Vapour}liquid equilibrium: ethanol}water, 760 mmHg.
Continuous line, bubble point line; dashed line, dew point line.
If a concentration greater than that represented by
point N is desired, a single pot cannot accomplish the
task (Figure 6). Suppose, however, that we set up an
apparatus whereby we constantly feed the Rrst pot as
described earlier, but now we condense the product
vapour and put it in another pot where it can be
distilled a second time. The concentration of the va-
pour from the second pot is represented by point X,
about 82% by weight ethanol. It can be seen that
adding more pots to this scheme would result in
higher and higher concentrations of ethanol in the
product. There is, however, a limit to this approach.
As the bubble point and dew point lines get closer
together, the increase in ethanol concentration per
added pot decreases. Eventually, these two lines
touch. The point at which these lines touch is called
an azeotrope. Azeotrope is a Greek word meaning
‘to boil together’. Literally, at this point additional
separation by conventional two-phase distillation is
impossible because the liquid- and vapour-phase con-
centrations are identical. In fact, even getting close to
the azeotrope requires more advanced distillation
practices than those commonly used in whisky produc-
tion.
By anology, it can be seen that the problem of
recovering the residual ethanol from the still bottoms
can also be accomplished through the use of addi-
tional distillation stages. In practice, however, the
distillation column is a more efRcient method of ac-
complishing these distillation tasks than multiple pot
stills. Single malt Scotch whisky makes use of mul-
tiple pot stills in the production of their Rnal distillate
in a manner similar to that described above.
The Continuous Beer Still
The Rrst distillation element in a multicomponent
whisky distillation system is commonly referred to as
III / WHISKY: DISTILLATION 4487
Figure 7 Cut-away of typical distillation column.
the beer still. The beer still consists of a cylindrical
shell and number of evenly spaced trays connected by
pipes called downcomers. Figure 7 shows a cut-away
view of the inside of a typical beer still. The liquid in
the still moves across the trays and down the down-
comers. The vapour in the still moves up the column
through holes in the tray and through the liquid. The
pressure of the vapour under each tray must be great
enough to allow the vapour to pass through the holes
and through the liquid to the next level up the tray
without allowing the liquid to drip through the holes
(Figure 8). Each time the vapour passes through the
liquid, the vapour gains ethanol concentration while
the liquid loses ethanol concentration. One tray is
roughly equal to one distillation in a pot similar to
that discussed earlier. Technically, the vapour con-
denses in the liquid of the tray above it, and gives off
its heat of vaporization. This heat of vaporization in
turn revaporizes a corresponding volume of vapour
which is richer in ethanol.
The still is conceptually divided into two sections,
the stripping section and the rectifying section. The
stripping section is the part of the still that is on and
below the feed-tray level. This section is referred to as
4488 III / WHISKY: DISTILLATION
Figure 8 Typical plate flow detail.
the stripping section, because here the residual alco-
hol is essentially stripped from the feed stream so that
the still bottoms have a negligible presence of ethanol.
The still must be designed not only to produce a spirit
of the desired proof, but also to limit base losses.
Typically, the stripping section has about 16}20
plates. The plates in this section must be designed to
minimize the likelihood of fouling due to the grain
residue being present here. Almost exclusively, sieve
trays are used for this purpose because they have
larger, less complex vapour openings and wider toler-
ances to help prevent plugging with grain particles.
The space between the trays must also be sufRciently
wide to prevent foam and other entrained liquid on
one tray from inSuencing the tray above it.
It is possible for grain particles in the feed to be
entrained in and carried upwards by the vapour pass-
ing through the feed tray. This can happen on any
tray in the stripping section, but it is most critical on
the feed tray. Various approaches have been utilized
to minimize this problem; almost all are mechanical
alterations to the still itself. The most common de-
entrainment device is the use of one additional sieve
tray immediately above the feed tray.
The rectifying section of the still is the part that is
above the feed tray. In this section, the alcohol is
concentrated to the desired product proof. Typically,
the rectifying section has between two and Rve plates.
The plates in this section are designed to cause more
efRcient commingling of the vapour with the liquid as
the vapour passes through the plate. Since solids are
no longer an issue, the contacting mechanisms can be
more intricate and tolerances closer in this section.
The plates in this section may also be more closely
spaced because foaming and entrainment are much
less of a problem here than in the stripping section.
The Beer Heater
As a rule of thumb, the conditions of the feed stream
to the still should match, as closely as possible, the
conditions on the tray to which the feed is introduced.
It has already been noted that the ethanol concentra-
tion of the feed stream is generally between 5 and 9%
by weight. The concentration can be closely predicted
from heat and material balance calculations where no
empirical data exist for a given feed stream. It has
also been noted that the feed tray is generally near the
18th plate. The feed tray location can also be pre-
dicted from detailed will design calculations. The
only problem that remains, then, is the feed temper-
ature. When fermentation is complete, the beer
temperature is generally about 343C. The feed tray
liquid temperature should be about 933C. Since the
vapour from the still generally has to be cooled and
condensed, it provides a convenient source of heat to
pre-heat the beer. Usually, the beer feed is passed
through a shell and tube-type heat exchanger with
large diameter tubes to help alleviate plugging. The
vapours from the still are on the shell side of the
exchanger.
The condensate from the beer heater is generally
returned to the still as reSux. ReSux is the liquid
returned to the top of the still. It alters the number of
trays required to perform the desired degree of separ-
ation as well as the tower cross-sectional area and the
heating and cooling loads required for vaporization
and condensation. ReSux is generally referred to as
a ratio of the liquid returned to the still versus prod-
uct collected. As the reSux ratio goes up, the number
of trays required to perform the separation goes
down, but the requisite heating and cooling loads go
up. At inRnite reSux, the minimum number of trays is
achieved, but the maximum heating and cooling
loads are required. At minimum reSux, an inRnite
number of trays is required for the separation, but
minimum energy requirements are achieved. An opti-
mum reSux ratio can be calculated and the beer
heater can be designed to provide that reSux.
A general rule of thumb for still design would
require that the reSux be introduced to the still on the
top plate because of its temperature and composition.
However, many distillers have made the decision to
enter the reSux lower down the column near the beer
feed plate for quality reasons. Additionally, the Rnal
distillation proof in whisky production is only partly
determined by economic considerations. Depending

on the type of whisky being produced, there are
generally governmentally prescribed maximum
ethanol concentrations which may be permitted dur-
ing the distillation process. In the case of bourbon, the
US Bureau of Alcohol, Tobacco, and Firearms pre-
scribes that the distillate may be taken from the still at
no higher than 160 proof (80% ethanol by volume).
Of utmost importance, however, are the organoleptic
considerations which go into the production par-
ameters for the whisky. Product taken off at a
lower proof retains more of the grain character, while
product taken off at a higher proof tends to have less
of the grain Savour constituents.
The Doubler
Many distillers utilize a doubler in their whisky distil-
lation process. The doubler is basically a pot still, like
the one discussed earlier. The doubler acts as one
additional distillation stage. It is used in practice for
Rnal proof adjustment and for product quality en-
hancement. There are two fundamentally different
ways of operating the doubler. The Rrst is called true
double distillation. In true double distillation, the still
vapours generally pass through the beer heater Rrst,
and then one or more condensers, so that the product
is completely condensed back to a liquid form. This
liquid is then charged to the doubler where it is heated
with steam coils and re-vaporized. The vapour from
the doubler is then condensed again and taken off as
product.
The doubler can also be operated as a thumper. In
this case, the doubler is Rtted with a large sparger.
The doubler is charged with liquid to a level just
above the sparger. The liquid is typically de-
mineralized water or the low proof tails cut from
a previous distillation.The vapour from the still Rrst
passes through the beer heater then through the spar-
ger in the doubler where it bubbles through the liquid.
As the vapour passes through the liquid in the doub-
ler, it Sash condenses and gives off its heat of vapor-
ization which, in turn, revaporizes a corresponding
volume of vapour which is richer in ethanol. The
thumper gets its name from the sound made as the
vapour condenses while passing through the liquid.
Finally, the ethanol-enriched vapour passes through
one or more condensers and is taken off as product.
Reboilers
Most beer stills are heated by direct steam injection
from a low pressure steam sparger located in the base
of the still. A reboiler is a type of heat exchanger
which permits the use of higher pressure steam than
a steam sparger will allow. There are several advant-
III / WHISKY: DISTILLATION 4489
ages to using a reboiler. First, it acts as one theoretical
plate in the distillation column. Second, it saves on
the amount of waste to be disposed of from the still
bottoms because it adds no water to the system.
However, reboilers are not generally used in
whisky production because they have a great tend-
ency to scorch the grain in the bottoms and, hence,
degrade the product quality. In other stills with no
grain residue, reboilers have been used quite success-
fully.
Process Control
Control of the continuous beer still is generally ac-
complished by means of three interrelated control
loops. These loops regulate the level of the liquid in
the bottom of the still, the Sow of steam into the
bottom of the still and the Sow of the beer feed near
the top of the still.
Typically, the liquid level in the bottom of the still
is sensed by a level transmitter which, in turn, regu-
lates a control valve on the discharge of a continuous-
ly running base level pump. Alternatively, in certain
conRgurations, the base level can be regulated very
simply by means of a Soat valve set at a certain level.
This requires that the discharge be capable of gravity
Sow away from the still bottom. Additionally, newer
technology has made it possible to dispense with the
control valve on the base level pump. The level trans-
mitter can provide a signal to a frequency inverter
which controls the frequency of the electrical current
running the pump. This frequency shift will cause the
pump to speed up or slow down in relation to the
signal from the level transmitter.
In a similar manner, the steam Sow to the still is
generally held at a constant base pressure or a con-
stant Sow rate. Base pressure control is the most
common means of steam control. A pressure trans-
mitter in the base of the still above the liquid level
provides a control signal to a control valve which, in
turn, regulates the Sow of low pressure steam into
the steam sparger in the bottom of the still. If steam
Sow control is desired, an oriRce plate or vortex Sow
meter is inserted into the steam line. The Sow-sensing
device provides the control signal to regulate the
control valve. In the past, some distillers have used
the still top temperature as a means of regulating the
steam Sow, while holding the beer feed constant.
While this means is effective, it tends to be less re-
liable due to the relatively large amount of process
response lag time.
The beer feed is generally regulated by means of
sensing the still top temperature, which is directly
related to the proof of the distillate. A temperature
transmitter generally provides a control signal to
4490 III / WINE: GAS AND LIQUID CHROMATOGRAPHY
a process control valve in the beer feed line, which is
fed by a constantly running feed pump. More recent
technology has made it possible to control the
proof more directly by using the temperature-correc-
ted density function of a mass Sow meter, which
can be correlated to the proof of the discharge
from the still. The only downside to the use of
a mass Sow meter is the process lag time that results
from having to measure the proof of the distillate
after condensation. Additionally, the control valve
can be eliminated from this loop by using a frequency
inverter, as described above. Some distillers employ
a more sophisticated means of controlling the beer
feed to the still by use of a cascaded control loop.
Typically, a magnetic Sow meter is used to measure
the Sow of beer to the still and control the operation
of the control valve. The still top temperature trans-
mitter provides a signal which is used to manipulate
the control settings for this Sow control loop.
In addition to the above controls, one or more
condensers must also be controlled. Generally, a con-
trol valve on the inlet cooling water line is used to
control this process. The control signal typically com-
es from a temperature transmitter which can either be
located on the discharge water line or the discharge
product line. Due to the relatively quick Sow rate of
the cooling water with respect to the product Sow
rate, process control response is generally much bet-
ter if the temperature transmitter is located on the
cooling water discharge line.
Finally, if the product is double-distilled in a true
doubler, one additional control loop is required. The
steam Sow to the steam coils inside the doubler
must be regulated. Almost without exception, this
loop consists of a steam control valve and a temper-
ature transmitter on the vapour discharge from the
doubler. In a manner similar to the still top control,
WINE: GAS AND LIQUID
CHROMATOGRAPHY
J. Guasch and O. Busto, Universitat Rovira i Virgili,
Tarragona, Spain
Copyright ^ 2000 Academic Press
Introduction
From the chemical point of view, wines are aqueous
alcoholic solutions containing more than 1000 com-
ponents that can be present at high concentrations
(g L\1), but also at trace levels (ng L\1). Some of
new technology has made it possible to control the
discharge proof more directly using a mass Sow meter.
Conclusion
A sign at the Stitzel-Weller distillery in Louisville,
Kentucky sums up the traditional view of the impact
of science on the beverage alcohol industry:
No Chemist Allowed
Nature and the oldtime know-how of the master distiller
get the job done here. Because traditional Kentucky
whisky is a natural product, we disdain synthetics, scien-
tist, and their accompanying apparatus. This is a distil-
lery, not a whisky factory.
Pappy Van Winkle
Tradition handed down through the generations is
the predominant means of whisky production. There
are numerous stories of a distiller who had to replace
his still because it had worn out. When the new still
was being installed, the distiller would make sure that
it was identical to the one it was replacing, right
down to the dent in the side of the still, which was
generally reapplied by the master distiller himself.
As a result, technological change is slow to be
adopted in an industry where any change in the pro-
cess may result in a changed taste. Technology is
gaining a foothold in the area of process control,
where new and better Rnal control elements, trans-
mitters and control systems are always being applied.
This traditional approach has also resulted in an
almost complete lack of published literature on the
topic of whisky distillation, which at best is viewed by
the industry as only part science and part art.
See Colour Plate 127.
See also: III/Wine: Gas and Liquid Chromatography.
these components determine the organoleptic proper-
ties of wines, while others are signi"cant for classify-
ing their origin and/or for checking whether some
adulteration has taken place. Concentration levels of
these compounds vary according to the variety of
vine, the climatic conditions under which the grapes
were grown, and the conditions under which vini"ca-
tion and ageing processes have been developed.
The quality of wines is established by sensory anal-
ysis, which is clearly correlated to their chemical